CN111908914B - Grain boundary layer ceramic material, preparation method and application of grain boundary layer ceramic substrate - Google Patents

Grain boundary layer ceramic material, preparation method and application of grain boundary layer ceramic substrate Download PDF

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CN111908914B
CN111908914B CN202010685817.2A CN202010685817A CN111908914B CN 111908914 B CN111908914 B CN 111908914B CN 202010685817 A CN202010685817 A CN 202010685817A CN 111908914 B CN111908914 B CN 111908914B
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boundary layer
grain boundary
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ceramic substrate
preparation
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CN111908914A (en
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冯毅龙
吕明
卢振亚
陈炜豪
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Guangzhou Tianji Electronic Technology Co ltd
South China University of Technology SCUT
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Guangzhou Tianji Electronic Technology Co ltd
South China University of Technology SCUT
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Abstract

The invention provides a grain boundary layer ceramic material, a preparation method and application of a grain boundary layer ceramic substrate, and belongs to the technical field of chip capacitors. The grain boundary layer ceramic material provided by the invention comprises the following preparation raw materials in parts by mass: SrTiO395.35 to 99.30 parts of Nb2O30.30-0.55 part of modified additive and 0.30-5.00 parts of modified additive; the modified additive is BaCO3、Nd2O3、CaO、Sm2O3、Al2O3And SiO2One or more of them. The grain boundary layer ceramic substrate prepared from the grain boundary layer ceramic material has excellent repeatability and consistency.

Description

Grain boundary layer ceramic material, preparation method and application of grain boundary layer ceramic substrate
Technical Field
The invention relates to the technical field of chip capacitors, in particular to a grain boundary layer ceramic material, a preparation method of a grain boundary layer ceramic substrate and application of the grain boundary layer ceramic substrate.
Background
In the national defense industry technology, the chip capacitor is more and more widely applied. The chip capacitor has a single-layer structure, and compared with an MLCC (multilayer ceramic capacitor), the chip capacitor has no current loop between dielectric layers, so that the chip capacitor has very low ESR (equivalent series resistance) and ESL (equivalent series inductance), and is particularly suitable for high-frequency application fields such as radar, navigation, satellite communication and the like.
The grain boundary layer ceramic material adopts SrTiO3The base material adopts AB site precise chemical doping to replace process, and has the features of high dielectric constant, stable temperature characteristic, excellent microwave characteristic, etc. The structure of the structure is shown in figure 1, and comprises a semi-conductive crystal grain, a grain boundary diffusion layer and a grain boundary insulating layer.
At present, certain problems exist in the electrical property and controllability of the ceramic material of the grain boundary layer, and the repeatability and consistency of the electrical property of the ceramic substrate of the grain boundary layer are further influenced.
Disclosure of Invention
The invention aims to provide a grain boundary layer ceramic material, a preparation method of a grain boundary layer ceramic substrate and application of the grain boundary layer ceramic substrate.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a grain boundary layer ceramic material which comprises the following preparation raw materials in parts by mass:
SrTiO395.35 to 99.30 parts of Nb2O30.30-0.55 part of modified additive and 0.30-5.00 parts of modified additive; the modified additive is BaCO3、Nd2O3、CaO、Sm2O3、Al2O3And SiO2One or more of them.
The invention provides a preparation method of a ceramic substrate with a grain boundary layer, which comprises the following steps:
mixing the grain boundary layer ceramic material, the adhesive and the organic solvent, and molding to obtain a membrane;
carrying out glue removal and reduction firing on the membrane by adopting a one-step method to obtain a semiconductive crystal grain ceramic substrate;
coating the surface of the semiconductive grain ceramic substrate with an oxidant dispersion liquid to obtain the semiconductive grain ceramic substrate attached with an oxide medium film;
and carrying out oxidation heat treatment on the semiconductive crystal grain ceramic substrate attached with the oxide medium film under the pure oxygen atmosphere to form a crystal boundary insulating layer, thereby obtaining the crystal boundary layer ceramic substrate.
Preferably, the adhesive is polyvinyl butyral and butyl benzyl phthalate, and the mass ratio of the polyvinyl butyral to the butyl benzyl phthalate is (3.0-5.0): (1.5-3.2).
Preferably, the organic solvent is xylene and absolute ethyl alcohol, and the mass ratio of the xylene to the absolute ethyl alcohol is (14.5-15.5): (14.5-15.5).
Preferably, the mass ratio of the grain boundary layer ceramic material to the polyvinyl butyral is (57.0-62.0): (3.0-5.0).
Preferably, the temperature range of the binder removal is 100-900 ℃, and the heating rate is 0.4-0.8 ℃/min in the process of heating from 100 ℃ to 900 ℃.
Preferably, the reduction firing temperature is 1380-1550 ℃, and the heat preservation time is 2-4 h.
Preferably, the oxidant in the oxidant dispersion liquid is one or more of substances containing B ions, Bi ions, Pb ions, Cu ions, Mo ions, Ni ions, Ti ions, Zn ions, Mg ions or Ca ions; the solvent of the oxidant dispersion liquid is one or more of terpineol, absolute ethyl alcohol and n-butyl alcohol; the mass ratio of the oxidant to the solvent in the oxidant dispersion liquid is 1: (1-1.5).
Preferably, the flow rate of pure oxygen used in the pure oxygen atmosphere is 1-5L/min, the temperature of the oxidation heat treatment is 850-1050 ℃, and the heat preservation time is 1.5-3.5 h.
The invention provides application of the grain boundary layer ceramic substrate prepared by the preparation method in the technical scheme in a chip capacitor.
The invention provides a grain boundary layer ceramic material which comprises the following preparation raw materials in parts by mass: SrTiO395.35 to 99.30 parts of Nb2O30.30-0.55 part of modified additive and 0.30-5.00 parts of modified additive; the modified additive is BaCO3、Nd2O3、CaO、Sm2O3、Al2O3And SiO2One or more of them. The invention uses SrTiO3Using Nb as a main raw material2O3As a semiconducting accelerator, SrTiO is accelerated3The semi-conduction in a reducing atmosphere forms crystal grains with low resistivity, so that the dielectric constant of the ceramic substrate of the grain boundary layer is improved; simultaneous utilization of BaCO3And Sm2O3Carry out Ba2+、Sm3+Co-doping modification can obtain SrTiO with huge dielectric constant and low dielectric loss under wide temperature and wide frequency3A base ceramic material; using Nd2O3With SrTiO3Compounding with Nd with high dielectric constant2O3The dielectric constant of the ceramic material is improved, and the electrical property of the ceramic material is further improved; using Al2O3And SiO2The method has the characteristics that the powder can form a molten state (namely a low-melting state) at a lower temperature, the firing temperature is reduced, and abnormal growth of crystal grains caused by overhigh firing temperature is avoided, so that the uniformity of the crystal grains and the electrical property of the ceramic material are improved, and the consistency of the electrical property of the ceramic substrate of the grain boundary layer is further ensured.
According to the invention, by adjusting the composition of the grain boundary layer ceramic material, the electrical property and the electrical property uniformity of the grain boundary layer ceramic material can be controlled, so that the grain boundary layer ceramic material has controllability.
The invention provides a preparation method of a ceramic substrate with a grain boundary layer, which directly adopts pure SrTiO3Replace SrCO in the prior art3With TiO2In the pre-synthesis process, incomplete reactants similar to free strontium are generated in the pre-synthesis process, so that the repeatability and consistency of substrate batches are poor; the invention has no pre-synthesis process, not only simplifies the process, but also ensures the repeatability of the processAnd consistency.
According to the invention, the one-step method is adopted for binder removal and reduction firing, so that the firing process is simplified, cooling is not required after binder removal, reduction firing is directly performed at high temperature, the crystal grains do not need to undergo the process of cooling and restarting, the demand for thermal efficiency is greatly reduced, the continuity of thermal efficiency is ensured, a uniform crystal boundary insulating layer is favorably formed, and a semiconductive crystal grain ceramic substrate with high electrical property repeatability and consistency is obtained. In the prior art, the binder removal and the reduction firing are carried out separately, the binder removal is carried out in the air, the reduction firing is carried out after cooling, because of the cooling process after the binder removal, the original pre-grown crystal grains lose a large amount of activity due to cooling, and the original activity of the crystal grains can be activated and reduced only by needing larger energy during the reduction firing, so that the prior art needs larger thermal efficiency, and the starting efficiency of each part of the substrate is inconsistent, which can influence the electrical property repeatability and consistency of the ceramic substrate.
The method adopts a mode of carrying out oxidation heat treatment under pure oxygen atmosphere to replace the existing mode of oxidation in air, is favorable for reducing the oxidation temperature and accelerating the oxidation rate of grain boundaries, improves the permeation degree of an oxidant, and is favorable for ensuring that the oxidant permeates all over the grain boundaries, thereby improving the electrical property repeatability and consistency of the ceramic substrate of the grain boundaries.
Drawings
FIG. 1 is a schematic structural diagram of a grain boundary layer ceramic material in the background art.
Detailed Description
The invention provides a grain boundary layer ceramic material which comprises the following preparation raw materials in parts by mass:
SrTiO395.35 to 99.30 parts of Nb2O30.30-0.55 part of modified additive and 0.30-5.00 parts of modified additive; the modified additive is BaCO3、Nd2O3、CaO、Sm2O、Al2O3And SiO2One or more of them.
In the present invention, unless otherwise specified, all the starting materials required for the preparation are commercially available products well known to those skilled in the art.
The preparation raw material of the grain boundary layer ceramic material comprises SrTiO395.35 to 99.30 parts, preferably 96 to 98 parts, and more preferably 96.5 to 97.5 parts. In the present invention, the SrTiO3The purity of (b) is preferably 98.9 to 99.6%. The invention uses SrTiO3As a basic raw material of the ceramic material, the ceramic material has the characteristics of high dielectric constant and low dielectric loss, and the electrical property of the ceramic material is ensured.
With said SrTiO3The preparation raw material of the grain boundary layer ceramic material comprises Nb2O30.30 to 0.55 part, preferably 0.35 to 0.50 part, and more preferably 0.40 to 0.45 part. The invention utilizes Nb2O3As a semiconducting accelerator, SrTiO is accelerated3The semiconductor is formed in a reducing atmosphere to form crystal grains with low resistivity, thereby improving the dielectric constant of the ceramic substrate of the grain boundary layer.
With said SrTiO3The preparation raw materials of the grain boundary layer ceramic material provided by the invention comprise 0.30-5.00 parts of modified additive, preferably 0.50-4.00 parts, more preferably 1.00-3.00 parts, and further preferably 1.50-2.50 parts by mass. In the invention, the modifying additive is BaCO3、Nd2O3、CaO、Sm2O3、Al2O3And SiO2More preferably BaCO3、Nd2O3、CaO、Sm2O3When the modifying additive is preferably one or more of the above, the proportion of the modifying additive of different types is not particularly limited, and any proportion can be adopted in the invention. The invention utilizes BaCO in the modified additive3And Sm2O3To SrTiO3Carry out Ba2+、Sm3+Co-doping modification can obtain SrTiO with huge dielectric constant and low dielectric loss under wide temperature and wide frequency3A base ceramic material; using Nd2O3With SrTiO3Compounding with Nd with high dielectric constant2O3To improve the dielectric constant of the ceramic material and further improve the ceramicElectrical properties of the porcelain material; using Al2O3And SiO2Can form low-solubility state and reduce the sintering temperature. The invention not only can effectively reduce the sintering temperature and promote the grain growth, but also can reduce the defects brought by the grain boundary and ensure the electrical property of the ceramic material by doping the proper amount of CaO.
In the invention, the preparation process of the grain boundary layer ceramic material is preferably to mix the SrTiO3、Nb2O3And the mixture of the modified additive is sequentially subjected to mixing, ball milling, drying and sieving to obtain the grain boundary layer ceramic material. The process of mixing, ball milling and drying is not particularly limited in the present invention and may be performed according to processes well known in the art.
In the present invention, the average particle diameter D of the grain boundary layer ceramic material50Preferably 0.4 to 0.7 μm. The sieving process is not particularly limited, and the particle size requirement can be met.
The invention provides a preparation method of a ceramic substrate with a grain boundary layer, which comprises the following steps:
mixing the grain boundary layer ceramic material, the adhesive and the organic solvent, and molding to obtain a membrane;
carrying out glue removal and reduction firing on the membrane by adopting a one-step method to obtain a semiconductive crystal grain ceramic substrate;
coating the surface of the semiconductive grain ceramic substrate with an oxidant dispersion liquid to obtain the semiconductive grain ceramic substrate attached with an oxide medium film;
and carrying out oxidation heat treatment on the semiconductive crystal grain ceramic substrate attached with the oxide medium film under the pure oxygen atmosphere to form a crystal boundary insulating layer, thereby obtaining the crystal boundary layer ceramic substrate.
The preparation method comprises the steps of mixing the grain boundary layer ceramic material, the adhesive and the organic solvent, and forming to obtain the membrane. In the invention, the adhesive is preferably polyvinyl butyral (PVB) and butyl benzyl phthalate, and the mass ratio of the polyvinyl butyral to the butyl benzyl phthalate is preferably (3.0-5.0): 1.5-3.2, more preferably (3.5-4.5): 1.8-3.0, and further preferably (3.8-4.2): 2.0-2.5. In the present invention, the polyvinyl butyral is preferably B-98; the butyl benzyl phthalate is preferably S-160.
In the invention, the organic solvent is preferably xylene and absolute ethyl alcohol, and the mass ratio of the xylene to the absolute ethyl alcohol is preferably (14.5-15.5): (14.5-15.5).
In the invention, the mass ratio of the grain boundary layer ceramic material to the polyvinyl butyral is preferably (57.0-62.0): (3.0-5.0), more preferably (58.0-61.0): (3.5-4.5), and further preferably (59.0-60.0): (3.8-4.2).
The process for mixing the grain boundary layer ceramic material, the adhesive and the organic solvent is not particularly limited, and the raw materials can be uniformly mixed according to the process well known in the art. In the present invention, the forming mode is preferably rolling or casting, and the specific process of the rolling or casting is not particularly limited, and may be performed according to a process well known in the art. After the forming is finished, the invention preferably cuts the membrane according to the actual required size. In the present invention, the thickness of the membrane is preferably 0.20 mm.
In the invention, the forming process is a physical process of mixing the grain boundary layer ceramic material, the adhesive and the organic solvent, and no chemical reaction occurs.
After the diaphragm is obtained, the diaphragm is subjected to glue removal and reduction firing by a one-step method to obtain the semiconductive crystal grain ceramic substrate. According to the invention, the membrane sheets are preferably stacked or potted in a single-sheet mode, put into an atmosphere furnace and then introduced with compressed air for glue removal. In the invention, the temperature range of the rubber discharge is preferably 100-900 ℃, and the heating rate is preferably 0.4-0.8 ℃/min, more preferably 0.6 ℃/min in the process of heating from 100 ℃ to 900 ℃. The invention can remove organic matters and organic solvents such as adhesives and the like completely through glue removal.
In the invention, the rubber discharging and the reduction firing are carried out by adopting a one-step method; the one-step method is that after the glue discharging is finished, the film after the glue discharging is arranged at 9Keeping the temperature at 00 ℃ for 1H, and then introducing a hydrogen-oxygen mixed gas (2-20% H) into the atmosphere furnace2) And then reduction firing is performed. The one-step method is corresponding to the process of step-by-step glue discharging and reduction firing in the prior art, and the prior art comprises the steps of firstly discharging glue in the air, cooling, then placing in an atmosphere furnace for reduction firing, namely, step-by-step glue discharging and reduction firing.
In the invention, the temperature of the reduction firing is preferably 1380-1550 ℃, more preferably 1400-1500 ℃, further preferably 1420-1460 ℃, and the heat preservation time is preferably 2-4 h, more preferably 2.5-3.5 h. In the reduction firing process, Nb2O3Fully solid-dissolved under the action of a reducing atmosphere and can be used as a donor to replace Ti4+，Nb5+The substituted solid solution weakens the bonding strength of oxygen and surrounding cations, promotes oxygen to be desorbed from the inherent lattice points and volatilizes to the outside, thereby forming semi-conductive crystal grains in the membrane, generates oxygen vacancies at the crystal grain boundary, and the oxygen vacancies are mainly distributed on the surfaces of the crystal grains.
After the semiconductive crystal grain ceramic substrate is obtained, the invention coats the surface of the semiconductive crystal grain ceramic substrate with the oxidant dispersion liquid to obtain the semiconductive crystal grain ceramic substrate attached with the oxidation medium film. In the present invention, the oxidizing agent in the oxidizing agent dispersion liquid is preferably one or more of substances containing B ions, Bi ions, Pb ions, Cu ions, Mo ions, Ni ions, Ti ions, Zn ions, Mg ions, or Ca ions, and more preferably Bi ions2O3、Bi(NO3)3、Cu(NO3)2、CuO、MgB、TiO2、ZnO、PbTiO3、Pb(ZrxTi1-x)O3、CaCu3Ti4O12、Ti(OC4H9)4And Bi2Mo3O12One or more of the above; when the oxidizing agent is preferably selected from the above substances, the ratio of the different oxidizing agents is not particularly limited, and any ratio can be used.
In the present invention, the solvent in the oxidant dispersion liquid is preferably one or more of terpineol, absolute ethyl alcohol and n-butanol. When the solvent in the oxidant dispersion liquid is preferably several of the above substances, the ratio of different solvents in the present invention is not particularly limited, and any ratio may be used. In the present invention, the mass ratio of the oxidizing agent to the solvent in the oxidizing agent dispersion liquid is preferably 1: (1 to 1.5), more preferably 1: (1.2-1.4). In the present invention, the oxidizer dispersion is preferably present in the form of a slurry.
In the present invention, the preparation method of the oxidant dispersion liquid is preferably one or more of wet ball milling, ultrasound and stirring. The process of ball milling, ultrasonic and stirring is not particularly limited in the present invention and may be performed according to a process well known in the art.
The coating process is not particularly limited in the present invention, and the oxide dispersion can be uniformly applied to the surface of the semiconductive grain ceramic substrate according to a process well known in the art.
In the invention, the thickness of the oxidation medium film is preferably 8-12 μm, and more preferably 9-10 μm.
After the semiconductive crystal grain ceramic substrate with the oxide medium film is obtained, the semiconductive crystal grain ceramic substrate with the oxide medium film is subjected to oxidation heat treatment under pure oxygen atmosphere to form a crystal boundary insulating layer, and the crystal boundary layer ceramic substrate is obtained. The present invention preferably performs the oxidative heat treatment in an atmospheric furnace. In the invention, the flow rate of pure oxygen used in the pure oxygen atmosphere is preferably 1-5L/min, more preferably 2-3L/min, the temperature of the oxidation heat treatment is preferably 850-1050 ℃, more preferably 900-1000 ℃, more preferably 950-980 ℃, and the heat preservation time is preferably 1.5-3.5 h, more preferably 2-3 h. In the oxidation heat treatment process, all the residual unoxidized metal ions on the surface of the oxidation dielectric film layer are converted into oxides; the melting point of the oxidant is low, and the oxidant is melted and converted into a liquid phase at high temperature; the grain boundary is a non-compact structure formed among the crystal grains, so that under the action of capillary force, the liquid-phase oxidant uniformly permeates the grain boundary to form a grain boundary insulating layer, and a grain boundary layer ceramic substrate is obtained; in addition, grain boundary oxidation can occur in the oxidation heat treatment process, namely oxygen ions (the oxygen ions are from pure oxygen and an oxidant) fill oxygen vacancies formed in the grain boundary.
The invention provides application of the grain boundary layer ceramic substrate prepared by the preparation method in the technical scheme in a chip capacitor. The method of application is not particularly limited in the present invention, and the grain boundary layer ceramic substrate may be applied to a chip capacitor according to a method well known in the art.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Preparing a grain boundary layer ceramic material: 98.95 parts by weight of SrTiO30.38 parts by weight of Nb2O30.36 parts by weight of SiO2And 0.32 part by weight of Sm2O3The mixture is ball-milled, dried and sieved in sequence to obtain ceramic powder with an average particle size D500.62 μm;
mixing 57.39 parts of grain boundary layer ceramic material, 14.51 parts of dimethylbenzene, 14.51 parts of absolute ethyl alcohol, PVB B-983.70 parts and BBP S-1603.09 parts, molding by adopting a tape casting method to obtain a membrane (the thickness is 0.20mm), and cutting the membrane according to the size required by a product;
filling the diaphragm into a pot in a single interlayer mode, filling the pot into an atmosphere furnace, introducing compressed air into a temperature curve of 100-900 ℃ (the heating rate is 0.6 ℃/min) for removing glue, keeping the temperature of 900 ℃ for 1H after removing glue, and introducing hydrogen-oxygen mixed atmosphere (5% H)2) Reducing and sintering at 1385 ℃ for 3h to obtain a semiconductive crystal grain ceramic substrate;
adding CuO serving as an oxidant into a mixed solvent of terpineol and absolute ethyl alcohol (the volume ratio of terpineol to absolute ethyl alcohol is 5:1), performing ultrasonic and ball milling to obtain an oxidant dispersion liquid (the mass ratio of CuO to the mixed solvent is 1: 1.1);
coating the oxidant dispersion liquid on the surface of the semiconductive crystal grain ceramic substrate to obtain the semiconductive crystal grain ceramic substrate attached with an oxidant dielectric film, wherein the thickness of the oxidant dielectric film is 11 microns;
and (3) putting the semiconductive grain ceramic substrate attached with the oxidation medium film into an atmosphere furnace, and introducing pure oxygen (the flow is 1.5L/min, the oxidation temperature is 900 ℃) to carry out oxidation heat treatment for 3 hours to obtain the grain boundary layer ceramic substrate.
Examples 2 to 4
According to the preparation method of the example 1, the grain boundary layer ceramic substrate is prepared by adopting the grain boundary layer ceramic material proportion, the firing temperature, the electrophoresis process parameters and the oxidation process shown in the following table 1, and the processes and the reagent dosage which are not listed in the table are the same as those of the example 1.
TABLE 1 parameters of examples 2 to 4
Figure BDA0002587524140000081
Figure BDA0002587524140000091
The grain boundary layer ceramic substrates prepared in examples 1 to 4 were cut into 2X 2mm pieces by sputtering a metal electrode2And (5) a chip, and measuring the electrical property of the chip. The dielectric constant of the grain boundary layer ceramic substrate samples prepared in examples 1 to 4 was calculated from K ═ 11.3Ct/S (K is the calculated dielectric constant, C is the measured capacitance, t is the substrate thickness, and S is the chip area). The uniformity of dielectric constant was calculated by sampling 10 samples from each of the four corners and the center of a 50X 50mm substrate, and the performance data are shown in Table 2.
TABLE 2 Performance data for grain boundary layer ceramic substrates prepared in examples 1-4
Figure BDA0002587524140000092
As can be seen from Table 2, the batch difference rate of the K values of the samples prepared in the embodiments 1 to 4 is less than or equal to 18%, and the batch difference rate of the K values of the samples prepared by the conventional process is about 20 to 25% (within the range of 50 x 50 mm), which indicates that the grain boundary layer ceramic material has excellent electrical properties, and the grain boundary layer ceramic substrate prepared from the ceramic material obviously improves the repeatability and consistency of dielectric constants, namely the electrical property repeatability and consistency of the grain boundary layer ceramic substrate.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (9)

1. The preparation method of the grain boundary layer ceramic substrate is characterized by comprising the following steps:
mixing the grain boundary layer ceramic material, an adhesive and an organic solvent, and forming to obtain a membrane; the grain boundary layer ceramic material comprises the following preparation raw materials in parts by mass:
SrTiO395.35 to 99.30 parts of Nb2O30.30-0.55 part of modified additive and 0.30-5.00 parts of modified additive; the modified additive is BaCO3、Nd2O3、CaO、Sm2O3、Al2O3And SiO2One or more of the above;
carrying out glue removal and reduction firing on the membrane by adopting a one-step method to obtain a semiconductive crystal grain ceramic substrate;
coating the surface of the semiconductive grain ceramic substrate with an oxidant dispersion liquid to obtain the semiconductive grain ceramic substrate attached with an oxide medium film;
and carrying out oxidation heat treatment on the semiconductive crystal grain ceramic substrate attached with the oxide medium film under the pure oxygen atmosphere to form a crystal boundary insulating layer, thereby obtaining the crystal boundary layer ceramic substrate.
2. The preparation method of claim 1, wherein the adhesive is polyvinyl butyral and butyl benzyl phthalate, and the mass ratio of the polyvinyl butyral to the butyl benzyl phthalate is (3.0-5.0): (1.5-3.2).
3. The method according to claim 1, wherein the organic solvent is xylene and absolute ethanol, and the mass ratio of the xylene to the absolute ethanol is (14.5-15.5): (14.5-15.5).
4. The preparation method of claim 2, wherein the mass ratio of the grain boundary layer ceramic material to the polyvinyl butyral is (57.0-62.0): (3.0-5.0).
5. The preparation method according to claim 1, wherein the temperature range of the binder removal is 100-900 ℃, and the heating rate is 0.4-0.8 ℃/min in the process of heating from 100 ℃ to 900 ℃.
6. The preparation method according to claim 1, wherein the reduction firing temperature is 1380-1550 ℃ and the holding time is 2-4 h.
7. The preparation method according to claim 1, wherein the oxidizing agent in the oxidizing agent dispersion liquid is one or more of substances containing B ions, Bi ions, Pb ions, Cu ions, Mo ions, Ni ions, Ti ions, Zn ions, Mg ions, or Ca ions; the solvent of the oxidant dispersion liquid is one or more of terpineol, absolute ethyl alcohol and n-butyl alcohol; the mass ratio of the oxidant to the solvent in the oxidant dispersion liquid is 1: (1-1.5).
8. The preparation method according to claim 1, wherein the flow rate of pure oxygen used in the pure oxygen atmosphere is 1-5L/min, the temperature of the oxidation heat treatment is 850-1050 ℃, and the holding time is 1.5-3.5 h.
9. The use of the ceramic substrate with grain boundary layer prepared by the preparation method of any one of claims 1 to 8 in chip capacitors.
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